干旱区生态环境知识资源中心(Arid): 淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究

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	淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究
其他题名	Determination of Phtlalic Acid Esters in Different Water Bodies in Huai'an by SPE-UHPLC-MS/MS and Study on Their Pollution Characteristics
	吴珺玮; 姚海波; 霍宗利; 赵怀荣; 宋鑫; 冯晓青
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2021
卷号	57 期号:5 页码:1001-4020
中文摘要	建立一种固相萃取(SPE)富集,超高效液相色谱-串联质谱法(UHPLC-MS/MS)检测水中6种痕量邻苯二甲酸酯类化合物[PAEs,包括邻苯二甲酸二(4-甲基-2-戊基)酯(BMPP)、邻苯二甲酸二己酯(DHXP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二(2-丁氧基)乙酯(DBEP)、邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二壬酯(DNP)]的方法。样品用Waters Oasis HLB SPE柱萃取,用Box-Behnken Design响应面设计优化水中PAEs提取的固相萃取条件:样品量为200 mL时,上样流量为3 mL·min~(-1),淋洗剂为9 mL的9%(体积分数)甲醇溶液,洗脱剂为6 mL甲醇和3 mL乙酸乙酯组成的混合溶液。洗脱液氮吹至近干,经甲醇复溶后过0.22mum有机滤膜,滤液供UHPLC-MS/MS分析。以Agilent Poroshell 120EC-C18色谱柱为固定相,以不同体积比的甲醇和水组成的混合溶液为流动相进行梯度洗脱,色谱分离后的PAEs进入MS/MS,在电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式下检测。结果显示:在优化的试验条件下,6种PAEs可在9 min内完成出峰,6种PAEs的质量浓度均在1~20mug·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.05~0.12mug·L~(-1)。对基质水样进行3个浓度水平的加标回收试验,所得回收率为79.2%~103%,测定值的相对标准偏差(n=6)为1.3%~9.2%。方法用于淮安市枯水期和丰水期出厂水、二次供水和末梢水的分析,研究了其污染特征,结果显示:6种PAEs均被不同程度地检出;枯水期水样中具有致癌风险的DEHP含量较高;丰水期水样中的DNP、 DCHP、DHXP含量较枯水期的高;丰水期水样中的PAEs含量高于枯水期的。按照美国环境保护署(EPA)暴露风险评价方法对枯水期水样中的DEHP进行健康风险评估,所得风险值1.2610~(-7) (女性)和1.0310~(-7)(男性)均低于EPA和其他国际组织规定的标准限值(10~(-4)~10~(-6))。
英文摘要	A method was developed for trace determination of PAEs(including BMPP,DHXP,DCHP, DBEP,DEHP,DNP)in water by SPE coupled with UHPLC-MS/MS.Waters Oasis HLB SPE column was selected for extraction of PAEs in water,and SPE conditions were optimized by Box-Behnken Design response surface design:when the water sample volume was 200 mL,flow rate of sample introduction of 3 mL·min~(-1),9 mL of 10% (volume fraction)methanol solution as rinsing solvent,a mixed solution composed of 6 mL of methanol and 3 mL of ethyl acetate as eluent.The collected eluate was blown to near dryness by nitrogen,then redissolved by methanol and filtered through 0.22mum organic filter membrane.The filtrate was analyzed by UHPLC-MS/MS. Agilent Poroshell 120EC-C18 chromatographic column was used as stationary phase,and the mixed solutions consisting of methanol and water with different volume ratios were used as mobile phase for gradient elution.The PAEs after chromatographic separation were introduced into MS/MS and detected under ESI+ and MRM modes. The results showed that 6PAEs could be completely detected within 9 min under the optimized test conditions. Linearity relationships between mass concentrations of 6PAEs and their respective peak areas were found in the same range of 1-20mug·L~(-1),with limits of detection in the range of 0.05-0.12mug·L~(-1).Recovery test on the actual sample was made by standard addition method in the 3 concentration levels,giving values of recovery ranged from 79.2%to 103%,and RSDs(n=6)of determined values ranged from 1.3%to 9.2%.The proposed method was used for determination of 6PAEs in source water,tap water and secondary water supply in Huai'an from the abundant water period and low water period,and the pollution characteristics of water bodies were studied.Results obtained showed as follows:all the 6 PAEs were detected in different degrees;the content of DEHP with carcinogenic risk was higher in water sample from low water period,and the contents of DNP,DCHP and DHXP were higher in water sample from abundant water period;the contents of PAEs in water sample from abundant water period were higher than those in water sample from low water period.According to the exposure risk assessment method of EPA,the health risk assessment of DEHP in water sample from low water period showed that the risk values of 1.2610~(-7)(for female)and 1.0310~(-7)(for male)were lower than the standard limits (10~(-4)-10~(-6))stipulated by EPA and other international organizations.
中文关键词	固相萃取 ; 超高效液相色谱-串联质谱法 ; 响应面设计 ; 邻苯二甲酸酯 ; 水体
英文关键词	SPE UHPLC-MS/MS response surface design phtlalic acid ester water body
类型	Article
语种	中文
国家	中国
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6987548
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/365152
作者单位	吴珺玮, 淮安市疾病预防控制中心;;淮安市突发公共卫生事件应急检测重点实验室, ;;淮安市突发公共卫生事件应急检测重点实验室, 淮安;;淮安, ;; 223001;;223001.; 姚海波, 淮安市疾病预防控制中心;;淮安市突发公共卫生事件应急检测重点实验室, ;;淮安市突发公共卫生事件应急检测重点实验室, 淮安;;淮安, ;; 223001;;223001.; 赵怀荣, 淮安市疾病预防控制中心;;淮安市突发公共卫生事件应急检测重点实验室, ;;淮安市突发公共卫生事件应急检测重点实验室, 淮安;;淮安, ;; 223001;;223001.; 宋鑫, 淮安市疾病预防控制中心;;淮安市突发公共卫生事件应急检测重点实验室, ;;淮安市突发公共卫生事件应急检测重点实验室, 淮安;;淮安, ;; 223001;;223001.; 冯晓青, 淮安市疾病预防控制中心;;淮安市突发公共卫生事件应急检测重点实验室, ;;淮安市突发公共卫生事件应急检测重点实验室, 淮安;;淮安, ;; 223001;;223001.; 霍宗利, 江苏省疾病预防控制中心, 南京, 江苏 210001, 中国.
推荐引用方式 GB/T 7714	吴珺玮,姚海波,霍宗利,等. 淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究[J],2021,57(5):1001-4020.
APA	吴珺玮,姚海波,霍宗利,赵怀荣,宋鑫,&冯晓青.(2021).淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究.理化检验. B, 化学分册,57(5),1001-4020.
MLA	吴珺玮,et al."淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究".理化检验. B, 化学分册 57.5(2021):1001-4020.